JPH10191940A - Improvement of quality of mozuku extract and mozuku extract - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain fucoidan-contg. extract which is substantially tasteless, odorless and pale and is useful for treatment of gastric diseases, etc., from mozuku (Nemacystus decipiens (SURINGAR) KUCHUCK) by subjecting the mozuku or its extraction liquid to a hydrogen peroxide treatment. SOLUTION: The fucoidan-contg. extract is obtd. from the mozuku by bringing hydrogen peroxide into reaction with mozuku algar substances or adding the hydrogen peroxide to the mozuku extraction liquid. The mozuku algar substances are further subjected to a refining treatment after the hydrogen peroxide treatment to remove impurity of low mol.wt., by which the extract having a high fucoidan content is obtd. The mozuku extract of purity preferable as food is obtd. by removing the trace hydrogen peroxide remaining after the hydrogen peroxide treatment by a catalase treatment.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a coloring or a strong seaweed flavor (an odor and smell peculiar to seaweed) which hinders the use of a mozuku extract containing fucoidan in foods and drinks to utilize its useful action. Mozuku extract removed or reduced,
And a method for treating a mozuku extract therefor.

[0002]

BACKGROUND OF THE INVENTION Polysaccharides containing fucose as the main constituent sugar
Fucoidan has an anti-ulcer effect and an inhibitory effect on the stomach wall of the harmful bacterium Helicobacter pylori.It can be added to foods and drinks to make it possible to take it on a daily basis to help prevent and treat gastric diseases. Expected (JP 7
-138166).

[0003] Since fucoidan is contained in a large amount in mozuku, a seaweed belonging to brown algae, it can be obtained relatively easily by a method such as hot water extraction of mozuku. However, the mozuku extract obtained by hot water extraction is sufficiently usable for the above-mentioned applications as it is in terms of the fucoidan content, but is strongly colored brown and has a strong smell and taste unique to seaweed.

[0004] It is not easy to solve the above-mentioned problems that hinder the use of mozuku extracts, and even if it is limited to decolorization, it is generally adopted in the food field for the purpose of decolorization, deodorization, and removal of unpleasant taste. Activated carbon, porous adsorption resin, ion exchange resin, electrodialysis, ultrafiltration, fractionation with ethanol, chlorite,
Treatment with sulfites, hyposulfites, pyrosulfites, etc., is almost ineffective.

[0005]

SUMMARY OF THE INVENTION An object of the present invention is to simply solve the above-mentioned problems in the case where a mozuku extract is to be added to a food and use it, and to have a substantially tasteless, odorless and light-colored one. It is an object of the present invention to provide a method for obtaining a modified fucoidan-containing extract from mozuku.

[0006]

Means for Solving the Problems According to the present invention, which has succeeded in achieving the above object, in obtaining an extract containing fucoidan from mozuku, the raw material mozuku or its extract is subjected to a hydrogen peroxide treatment. It is characterized in that a purification treatment for removing low molecular weight impurities is performed as necessary.

[0007] A trace amount of hydrogen peroxide remaining after the hydrogen peroxide treatment is completely decomposed by catalase treatment as required.

[0008]

BEST MODE FOR CARRYING OUT THE INVENTION The mozuku extract to be improved in quality according to the present invention is obtained by subjecting mozuku to an extraction treatment with hot water, and concentrating and drying the obtained extract.

The step of extracting fucoidan with hot water can be carried out under any conditions by any method, such as the method described in the above-mentioned JP-A-7-138166. This is an extraction using hot water (referred to as an acid extraction method in the above publication). That is, mozuku alga bodies (in the case of salted products, those previously immersed in water and desalted) are suspended in about 1 to 3 times the wet weight of water, and diluted hydrochloric acid, acetic acid and the like are added to adjust the pH. After adjusting to 2-4, preferably 2-3, about 50 ° C. or more, preferably about 8
Heat to 0-100 ° C to elute fucoidan. Subsequently, the precipitate is removed by centrifugation, and the supernatant is neutralized with a sodium hydroxide solution.

The extract obtained by this method contains about 10 to 40% by weight of fucoidan per solid.

The hydrogen peroxide treatment according to the present invention is carried out by adding hydrogen peroxide to this extract or applying to the mozuku algae to be subjected to the extraction treatment. The extract can be subjected to any purification treatment before the treatment with hydrogen peroxide.

[0012] When the mozuku alga body is treated with hydrogen peroxide,
In a state where the concentration of hydrogen peroxide is about 100 to 500 mM and about 0.3 to 3.4% by weight based on the raw material mozuku,
It is desirable to carry out the reaction at a pH of about 5 to 7 and a temperature of about 20 to 40 ° C. After the treatment, solid-liquid separation is performed, and the separated algal cells are subjected to an extraction treatment. Since a considerable amount of fucoidan (treated with hydrogen peroxide) is eluted in the liquid phase separated by the solid-liquid separation operation after the hydrogen peroxide treatment, fucoidan can be recovered therefrom. .

When the original algal extract is treated with hydrogen peroxide, the preferable treatment conditions vary depending on the concentration of the extract, etc., but the extract is obtained by extracting the extract with the same amount of hot water as the mozuku alga body. If present, the concentration of hydrogen peroxide in the reaction system is about 100 to 5
00 mM (about 0.6 to 3% by weight based on the raw material mozuku), and the pH is adjusted to about 5 to 7 to about 20 to 4%.
It is desirable to react at 0 ° C.

The low molecular weight water-soluble components extracted from mozuku together with fucoidan, especially those causing color and seaweed flavor, are presumed to be largely decomposed into light-colored, tasteless and odorless substances by hydrogen peroxide treatment. The coloring of the extract and the seaweed flavor are significantly reduced.

If a small amount of hydrogen peroxide used in the treatment remains, it is not preferable when the mozuku extract is used for foods. Therefore, if necessary, catalase (EC 1.1.
Process in step 1.6) to completely decompose. An example of a commercially available enzyme preparation that can be used is Catazyme 50L (a product of Novo Nordisk Bioindustry).

The treatment with hydrogen peroxide does not cause decomposition of fucoidan, and the treatment with hydrogen peroxide does not adversely affect the yield and quality of fucoidan.

The mozuku extract after the hydrogen peroxide treatment and the extract obtained from the mozuku treated with the hydrogen peroxide generally contain unnecessary salts and low molecular weight water-soluble components. If these insoluble components are removed by ultrafiltration, electrodialysis, etc., an extract having a high fucoidan content can be obtained.

The fucoidan extract obtained by the treatment with hydrogen peroxide according to the present invention has little coloring and seaweed flavor, so it can be arbitrarily added to various foods and drinks without fear of deteriorating the original taste of the foods and drinks. To take advantage of fucoidan's useful effects.

[0019]

【Example】

EXPERIMENTAL EXAMPLE 1 1 kg of Okinawan salted mozuku (hereinafter referred to as "raw algae") was immersed in three times the amount of water to desalinate, 1 liter of water was added, and the pH was adjusted to 3 with hydrochloric acid. Next, the mixture was heated to 90 to 95 ° C. for 60 minutes, cooled, and centrifuged to obtain an extract containing fucoidan.

Hydrogen peroxide (hydrogen peroxide content 35%) was added from 10 mM to 1 M (340 ppm to 34,
000ppm) at 4 ° C or 30 ° C.
Allowed to react for hours. After the treatment, the remaining hydrogen peroxide was decomposed by adding 1,000 units of catalase (catazyme 50 L).

Table 1 shows the decolorization rate by the above treatment. The decolorization rate is a value calculated from the change in the absorbance at 520 nm measured for the extract (solid content concentration: about 2.5% by weight) according to the following equation. The concentration is corrected for the absorbance of the extract of Example 1. The decolorization rate in each of the following examples is a value measured in the same manner.)

Decolorization ratio (%) = [(absorbance before treatment−absorbance after treatment) / absorbance before treatment] × 100

[0023]

[Table 1] Decolorization rate by hydrogen peroxide treatment (%) Hydrogen peroxide concentration (mM) Treatment temperature 4 ° C Treatment temperature 30 ° C 10 0 17.4 21 4.4 24.3 31 6.0 28.3 51 8.5 34.5 103 12.4 43.6 206 17.7 53.5 309 21.1 59.0 515 25.5 65.5 1029 32.3 73.8

From Table 1, it can be seen that the concentration of hydrogen peroxide was about 100 mM.
It can be seen that remarkable decolorization is performed by the above processing.

EXPERIMENTAL EXAMPLE 2 p of reaction system when treating Mozuku extract with hydrogen peroxide
The effect of H and temperature on the decolorization rate was investigated. The mozuku extract used in the experiment is the same as that used in Experimental Example 1. The pH of the mozuku extract is adjusted to about 3 to 8 by adding hydrochloric acid or sodium hydroxide, and to 30 ml of the extract, hydrogen peroxide is added to a concentration of about 100 mM to 1 M.
Alternatively, the reaction was carried out at 30 ° C. for 17 hours. Subsequently, 1,000 units of catalase were added to decompose and remove excess hydrogen peroxide. Table 2 shows the results.

The decolorization rate was better at higher hydrogen peroxide concentrations and higher reaction temperatures at all hydrogen peroxide concentrations.

[0027]

TABLE 2 Effect of hydrogen peroxide treatment conditions on decolorization rate reaction temperature _{H 2 O 2 H 2 O 2} H 2 O 2 H 2 O 2 initial pH (℃) 100mM 210mM 520mM 1030mM 3.11 4 13% 18% 29% 39% 〃30 45 55 68 76 5.00 00 429 37 50 60 ３０30 68 877 85 88 6.02 434 342 354 64 ３０30 72 79 79 90 90 7.02 439 48 58 68 ３０30 75 81 81 88 91 8.02 4 44 52 62 62 71 ３０ 30 77 83 89 92

Comparative Example 1 2 kg of original algae were immersed in 3 times the amount of tap water for desalting. Then, the same amount of tap water as the original algae was added, and the pH was adjusted to 3 with sulfuric acid. For 60 minutes. After cooling, the solid matter was removed by centrifugation, and the extract 34 containing fucoidan was removed.
20 ml were obtained.

[0029] A half of this extract was subjected to pressure filtration using a polyacrylonitrile-based hollow fiber type ultrafiltration membrane, AIP1010 (fraction molecular weight: 6,000, Asahi Kasei Kogyo Co., Ltd.) to remove a low molecular fraction. Removed. Furthermore, 2 liters of deionized water is added to the fucoidan-enriched fraction, and
After adjusting H to 3, pressure filtration using the ultrafiltration membrane was performed. This operation was repeated three times in total.

Next, 2 liters of deionized water was added to the concentrated solution, followed by pressure filtration. After this operation was repeated twice, the mixture was concentrated under reduced pressure, freeze-dried, and powdered.

21.8 g of a brownish powder containing 74.2% by weight of fucoidan was obtained. The powder had a flavor unique to seaweed, and the decolorization ratio by the above purification was 8.4%.

Example 1 The pH of 1710 ml of the extract prepared in Comparative Example 1 was adjusted to 6 with sodium hydroxide, and 35% aqueous hydrogen peroxide was added so that the concentration in the reaction system became 490 mM.
For 17 hours.

Then, 17,100 units of catalase were added to add 3
The mixture was allowed to act at 0 ° C. for 3 hours to decompose residual hydrogen peroxide. Then, the mixture was heated at 80 ° C. for 10 minutes to inactivate catalase, and further filtered to remove denatured proteins. The obtained hydrogen peroxide-treated mozuku extract has a decolorization rate of 80.0%.
It was pale. This was purified by the same ultrafiltration method as in Comparative Example 1 and freeze-dried to obtain 22.8 g of a slightly yellow powder containing 73.0% by weight of fucoidan (decolorization rate: 84%). This powder was tasteless and odorless.

Example 2 The pH of 1790 ml of an extract obtained by extracting mozuku in the same manner as in Comparative Example 1 was adjusted to 6 with sodium hydroxide, and then 55 ml of 31% hydrogen peroxide solution was added to the reaction system. At a hydrogen peroxide concentration of 270 mM, at 30 ° C.
Time acted.

After the treatment, 10,000 units of catalase were added and allowed to act at 30 ° C. for 3 hours to decompose the remaining hydrogen peroxide. Thereafter, the enzyme was inactivated by heating at 90 ° C. for 10 minutes, followed by filtration to remove denatured proteins. The mozuku extract after the treatment was light brown, and the decolorization ratio was 81.0%.

Next, the same ultrafiltration and washing as in Comparative Example 1 were carried out using a polysulfone-based ultrafiltration membrane having a molecular weight cutoff of 6,000 (SIP1013, Asahi Kasei Kogyo).

The purified fraction thus obtained was purified with sodium hydroxide.
Neutralized to H5.8, concentrated under reduced pressure and lyophilized to give a pale yellow, tasteless and odorless fucoidan content of 8
A powder of 0.1% by weight was obtained (bleaching rate 81.0%).

Example 3 1 kg of original algae was immersed in 3 times the volume of water for 30 minutes to desalinate, and then 100 ml of 35% hydrogen peroxide (1 mol, 1 mol,
(3.5% against original algae) and 1 liter of tap water, and the mixture was treated at 30 ° C. for 20 hours.

After the treatment, 2 liters of tap water was added, and 12
A viscous aqueous phase (hereinafter referred to as a solubilized fraction) and algal cells were separated using a mesh sieve. The separated solubilized fraction and algal cells were each treated with 5000 units of catalase.

The solubilized fraction weighed 9.12 g (23.8% solids)
% Of fucoidan (45.7% by weight of fucoidan in the original algae) and was well decolorized.

The alga bodies were heated under sulfuric acid at pH 3 for 60 minutes to extract fucoidan. The obtained extract contained 9.45 g of fucoidan (38.9% by weight based on solid content, 47.3% by weight of fucoidan in the original algae), and the decolorization rate was 80.0%.

The above-mentioned solubilized fraction and extract were subjected to the same purification treatment as in Comparative Example 1, and both were tasteless and odorless.
A white powder was obtained. The recoveries for fucoidan in the original algae were 42.0% and 39.2%, respectively.

Example 4 The purified extract obtained in Comparative Example 1 having a decolorization ratio of 8.4% was dissolved in water and treated with hydrogen peroxide at 30 ° C. for 20 hours.
Further, catalase treatment, filtration, concentration and drying were performed to obtain a tasteless and odorless powder having a fucoidan content of 75.7% by weight and a decolorization rate of 85.0%.

[0044]

As described above, the present invention is extremely effective for eliminating the coloring and the seaweed flavor of the mozuku extract, and facilitates the use of the mozuku extract in the food field.

Continued on the front page (51) Int.Cl. ⁶ Identification code FI C08B 37/00 C08B 37/00 G (72) Inventor Shusuke Hashimoto 1-1-19 Higashi-Shimbashi, Minato-ku, Tokyo Yakult Co., Ltd. (72 Inventor Teruo Yokokura 1-1-19 Higashishimbashi, Minato-ku, Tokyo

Claims (4)

[Claims] 1. A method for improving the quality of a fucoidan-containing mozuku extract, comprising subjecting the raw material mozuku or an extract thereof to hydrogen peroxide treatment in obtaining a fucoidan-containing extract from mozuku. 2. A method for obtaining an extract containing fucoidan from mozuku, comprising subjecting the mozuku as a raw material or an extract thereof to a hydrogen peroxide treatment, and then subjecting the mozuku to a purification treatment for removing low molecular weight impurities. A method for improving the quality of a mozuku extract containing. 3. The method for improving the quality of a mozuku extract according to claim 1, wherein a catalase treatment is performed after the hydrogen peroxide treatment. 4. A mozuku extract which has been subjected to a quality improvement treatment by the method according to any one of claims 1 to 3.